JPS6168122A - Recovering method of dimethylformamide - Google Patents
Recovering method of dimethylformamideInfo
- Publication number
- JPS6168122A JPS6168122A JP59188896A JP18889684A JPS6168122A JP S6168122 A JPS6168122 A JP S6168122A JP 59188896 A JP59188896 A JP 59188896A JP 18889684 A JP18889684 A JP 18889684A JP S6168122 A JPS6168122 A JP S6168122A
- Authority
- JP
- Japan
- Prior art keywords
- activated carbon
- dmf
- steam
- acf
- dimethylformamide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treating Waste Gases (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、ジメチルホルムアミド（以下ＤＭＦと記す）
含有排ガスから繊維状活性炭（以下ＡＣＦと記す）を用
いてＤＭＦを回収する方法に関するものである。Detailed Description of the Invention (Industrial Field of Application) The present invention relates to dimethylformamide (hereinafter referred to as DMF)
The present invention relates to a method for recovering DMF from contained exhaust gas using fibrous activated carbon (hereinafter referred to as ACF).
ＤＭＦは優れた有機溶媒であって、ＤＭＦ単独又はメチ
ルエチルケトン（以下ＭＥＫと記す）、トルエンなどの
有機溶媒と共に広く用いられており、乾燥機等より発生
するこれら有機溶媒含有排ガスから、これら有機溶媒を
捕捉回収することは環境対策上及び経済上からも必要で
ある。DMF is an excellent organic solvent and is widely used alone or together with organic solvents such as methyl ethyl ketone (hereinafter referred to as MEK) and toluene. Capturing and recovering is necessary from both environmental and economical points of view.
一般に気相系の有機溶媒を回収する方法として、活性炭
を利用する方法は広く行われており、有効な方法の一つ
である。Generally, as a method for recovering gas-phase organic solvents, a method using activated carbon is widely practiced and is one of the effective methods.
しかしながら、ＤＭＦを活性炭に吸着させ直接スチーム
再生し、ＤＭＦを回収する方法は行われていない。これ
は、ＤＭＦを吸着した活性炭をスチーム脱着する場合、
活性炭の再生可能温度にまでスチーム温度を高くすると
ＤＭＦが分解し、安定回収できず、ＤＭＦが分解しない
温度では、活性炭の再生ができないためである。However, no method has been used to recover DMF by adsorbing DMF onto activated carbon and directly regenerating it with steam. This is when steam desorption is performed on activated carbon that has adsorbed DMF.
This is because if the steam temperature is raised to a temperature at which activated carbon can be regenerated, DMF decomposes and cannot be stably recovered, and activated carbon cannot be regenerated at a temperature at which DMF does not decompose.
環境対策上の問題からＤＭＦを活性炭に吸着させた場合
には再生時ＤＭＦは分解廃棄されていた。Due to environmental concerns, when DMF is adsorbed onto activated carbon, the DMF is decomposed and disposed of during regeneration.
最近開発、実用化されｌＣＡ ＣＦは排ガス中の低濃度
有機溶媒の好適な吸着材として広く用いられている。こ
のＡＣＦに、排ガス中のＤＭＦを吸着させた場合、上記
活性炭の場合と同様な問題が懸念され、しかもＡＣＦが
活性炭に較べ高価であることと相俟って、ＡＣＦにＤＭ
Ｆを直接吸着させることは行わず、予め活性炭にて吸着
捕捉し、次いで他の有機溶媒はＡＣＦへの吸着及び脱着
によって回収され、活性炭に吸着した［）ＭＦは、活性
炭の再賦活の１ｌＩｉ廃棄されているのが現状である。Recently developed and put into practical use, lCA CF is widely used as a suitable adsorbent for low concentration organic solvents in exhaust gas. If this ACF were to adsorb DMF in the exhaust gas, there would be concerns about the same problems as in the case of activated carbon, and in addition, ACF is more expensive than activated carbon.
F is not directly adsorbed, but is adsorbed and captured in advance with activated carbon, and then other organic solvents are recovered by adsorption and desorption to ACF. This is the current situation.
本発明者はこのような問題を解決し、排ガス中のＤＭＦ
を、効率よく回収する方法を検討の結果本発明に至った
。The inventor of the present invention has solved such problems and
The present invention was developed as a result of research into a method for efficiently recovering .
（発明の構成〕
本発明は、ＤＭＦを含む排ガス中からＤＭＦを回収する
に当り、該排ガスをＡＣＦ吸着層に通してＤＭＦを吸着
除去し、清浄空気として放出すると共に、ＤＭＦに吸着
したＡＣＦを１６０〜２００℃の水蒸気にて脱着するこ
とを特徴とするＤＭＦの回収方法である。(Structure of the Invention) In recovering DMF from exhaust gas containing DMF, the present invention passes the exhaust gas through an ACF adsorption layer to adsorb and remove DMF, and releases it as clean air. This is a DMF recovery method characterized by desorption using water vapor at 160 to 200°C.
本発明によるとＡＣＦを用いてＤＭＦの脱着としては考
えられない高温において脱着プることによって、排ガス
中から効率よ＜ＤＭＦの回収が可能であると共に、ＡＣ
Ｆの吸着性能を低下させることなく再生することができ
るものである。According to the present invention, it is possible to efficiently recover DMF from exhaust gas by using ACF to desorb DMF at a high temperature that is unthinkable for desorption of DMF.
It can be regenerated without reducing F adsorption performance.
本発明において処理の対象とされる排ガスはＤＭＦの外
にＭＥＫ１トルエン、酢酸エチルなどの有機溶媒ガスを
含む混合ガスであることもできる。The exhaust gas to be treated in the present invention can also be a mixed gas containing organic solvent gas such as MEK1 toluene and ethyl acetate in addition to DMF.
本発明において用いられるＡＣＦは既知の八〇Ｆ、例え
ばレーヨン系ＡＣＦ、アクリル系へ〇Ｆ、フェノール系
ＡＣＦなどであるが、ＤＭＦはアミド系であるため比表
面積３００〜３０００ｍ’ ／Ｑのアクリル系ＡＣＦが
ＤＭＦに対し、特に高い吸着能を示し、このものを使用
するとＡＣＦ＠着缶の容積が小さくなり、その結果速か
な脱着が行われ高い回収率でＤＭＦを回収できる。The ACF used in the present invention is a known 80F, such as rayon-based ACF, acrylic-based ○F, phenol-based ACF, etc., but DMF is an amide-based acrylic-based ACF with a specific surface area of 300 to 3000 m'/Q. ACF exhibits a particularly high adsorption capacity for DMF, and when it is used, the volume of the ACF@adsorption can is reduced, resulting in rapid desorption and recovery of DMF at a high recovery rate.
本発明においては、ＡＣＦによってＤＭＦを吸着除去さ
れた排ガスは清浄空気として放出されると共に、ＤＭＦ
を吸着したＡＣＦは１６０〜２００℃のスチームで脱着
処理される。温度が１６０℃未満の場合には、繰返し使
用によって徐々にＡＣＦの吸着能（比表面積により評価
される）が低下し、また２００℃超の場合はＤＭＦの回
収率が低下する（後掲第１表参照）。In the present invention, the exhaust gas from which DMF has been adsorbed and removed by the ACF is released as clean air, and the DMF
The adsorbed ACF is desorbed using steam at 160 to 200°C. If the temperature is less than 160°C, the adsorption capacity of ACF (evaluated by specific surface area) will gradually decrease with repeated use, and if the temperature is over 200°C, the recovery rate of DMF will decrease (see Section 1 below). (see table).
ＡＣＦ吸着層の構造としてはＡＣＦのフェルト、織物、
または繊維状のまま支持体にて円筒状に固定された構造
とし、使用するのがよい。The structure of the ACF adsorption layer is ACF felt, woven fabric,
Alternatively, it is preferable to use a structure in which the fibers are fixed in a cylindrical shape with a support.
このようなＡＣＦ吸着層を装着したＡＣＦ吸着塔として
は第１図に示された装置とするのがよい。As an ACF adsorption tower equipped with such an ACF adsorption layer, the apparatus shown in FIG. 1 is preferable.
第１図は、ＡＣＦｅ着塔の断面図を示すものである。第
１図において１は排ガスの供給口であり、弁機構を有す
る入口部２かう、吸着缶３内に供給される。吸着缶３内
には円筒状ＡＣＦ吸着層４が配されており、缶内に供給
された排ガスは、この円筒状ＡＣＦ吸着層を通り、清浄
ガスとして排出口５を経て缶外に排出される。図中矢印
６はガスの流動方向を示す。FIG. 1 shows a cross-sectional view of an ACFe deposition tower. In FIG. 1, reference numeral 1 denotes a supply port for exhaust gas, which is supplied into an adsorption canister 3 through an inlet portion 2 having a valve mechanism. A cylindrical ACF adsorption layer 4 is disposed inside the adsorption can 3, and the exhaust gas supplied into the can passes through this cylindrical ACF adsorption layer and is discharged as clean gas to the outside of the can via an outlet 5. . Arrow 6 in the figure indicates the direction of gas flow.
一方、脱着用水蒸気はスチーム供給管７から缶内に供給
噴出され、ＡＣＦ吸着層４を通り、＠着されている有機
溶姪を脱着後、弁ｔａｇ ２を経て１２看蒸気８として
取出され、ＡＣＦ吸着層４は再生される。脱着蒸気８は
凝縮工程を経て、既知の方法にて、各含有成分毎に分離
される。On the other hand, the steam for desorption is supplied and ejected into the can from the steam supply pipe 7, passes through the ACF adsorption layer 4, desorbs the attached organic melt, and is then taken out as steam 8 through the valve tag 2. The ACF adsorption layer 4 is regenerated. The desorbed vapor 8 undergoes a condensation step and is separated into each component by a known method.
以上の如き脱着−脱着装置によると、ＡＣＦ吸着層の下
部から高温のスチームが供給されることとなるため、Ａ
ＣＦ＠着層の有効な活用が可能となる。According to the desorption-desorption device as described above, high-temperature steam is supplied from the lower part of the ACF adsorption layer.
Effective use of CF@adhesion layer becomes possible.
本発明において、供給される排ガスはＤＭＦを含むガス
であって、その濃度は特に制限されないが、ＤＭＦＩＮ
度が特に高い場合、あるいは排ガス中に繊維屑などの固
形物、高分子物質などが含まれる場合は、予めスクラバ
ー水洗処理してのちＡＣＦ吸着層に供給するのがよく、
スクラバー水洗処理によって水に溶解したＤＭＦは既知
の方法によって回収される。In the present invention, the exhaust gas to be supplied is a gas containing DMF, and its concentration is not particularly limited.
If the concentration is particularly high, or if the exhaust gas contains solid matter such as fiber waste, polymeric substances, etc., it is best to wash the scrubber with water before supplying it to the ACF adsorption layer.
DMF dissolved in water by the scrubber washing process is recovered by known methods.
本発明の実施に際して、例えば混合布Ｉ幾溶媒含有排ガ
スで、ＤＭＦ比が低い場合、これら混合有機溶媒を吸着
したＡＣＦの脱着は、毎回本発明方法を適用する必要は
なく、ＤＭＦの吸着缶が蓄積し、ＡＣＦの吸着能力が低
下したときに適用すればよい。When carrying out the present invention, for example, when the DMF ratio is low in a mixed cloth I mixed solvent-containing exhaust gas, it is not necessary to apply the method of the present invention every time to desorb ACF that has adsorbed these mixed organic solvents, and the DMF adsorption can is used. It may be applied when the adsorption capacity of ACF decreases due to accumulation.
例えばＭＥＫが含まれる場合１２０℃のスチームでの脱
着が充分可能であり、その方がエネルギーコスト的にも
好ましい。For example, when MEK is included, it is possible to fully desorb it with steam at 120° C., which is preferable in terms of energy cost.
（発明の効果〕
本発明方法によると、１６０〜２００℃特に１７０〜１
９０℃の水蒸気を用い、ＡＣＦに吸着したＤＭＦを脱着
することによって、第１表に示した通り、繰返し使用に
よっても、ＡＣＦの吸着能は低下せず、しかも高い収率
でＤＭＦを回収することができる。(Effects of the invention) According to the method of the present invention, temperature of 160 to 200℃, especially 170 to 1
By desorbing DMF adsorbed on ACF using water vapor at 90°C, as shown in Table 1, the adsorption capacity of ACF does not decrease even with repeated use, and DMF can be recovered in high yield. I can do it.
第 １ 表
注（１）実験方法： Ｄ Ｍ Ｆ １３００ｐｐｍを含
む排ガスをＡＣＦｍ着層に通してＤＭＦを吸着させ表に
記載のスチームにて脱着した。Table 1 Note (1) Experimental method: Exhaust gas containing 1300 ppm of DMF was passed through an ACFm deposition layer to adsorb DMF, and desorbed using steam as described in the table.
このときの供給盪と凝縮水溶液中のＤＭＦｌｉ度とより
求めた。It was determined from the supply rate at this time and the degree of DMFli in the condensed aqueous solution.
注（２）Ｎｏ■、■２■は本発明例、Ｎ ｏｌ、５は比
較例
本発明において再生したＡＣＦの比表面積は１２８０１
１’ ／ｇ 、１３００ｍ ’ ／Ｑで当初の比表面積
の約９５％を維持した。Note (2) No. ■, ■2■ are examples of the present invention, No. 1, 5 are comparative examples. The specific surface area of the ACF regenerated in the present invention is 12801
About 95% of the original specific surface area was maintained at 1'/g and 1300 m'/Q.
同様の操作を５ 、０００回繰返したがＡＣＦの比表面
積の低下は見られなかった。Although the same operation was repeated 5,000 times, no decrease in the specific surface area of ACF was observed.
脱＠温度を１３５℃で行った場合はサイクル時間が次第
に短くなり５００回目頃より半分の時間で破過するよう
になり回収率も低下し実用的でなくなった。When the de@-temperature was carried out at 135° C., the cycle time gradually became shorter, and from around the 500th cycle, the cycle time reached a breakthrough in half the time, and the recovery rate also decreased, making it impractical.
実施例
Ｄ Ｍ Ｆ １２００ｐｐｍ％Ｍ Ｅ Ｋ ２８００Ｅ
）Ｉ）ＩＲ１トルエン１１０００ｐｐ １酢酸エチル１
３０ｐｐｍを含むモデル排ガスを、比表面積１２００ｍ
’ ／（Ｊのアクリル系ＡＣＦフェルト３ｋｇを円筒
状に充填した第１図に示すＡＣＦＣＦｍ着層１１１１／
分にて供給した。このとき、ＡＣＦＣＦｍ着層排出され
るガス中の各成分の含有量は何れも１０ｐｐｍ以下であ
ったのでこのまま大気中に放出した。排出されるガス中
のＭＥＫ含有量が１０ｐｐｍを越える直前にモデル排ガ
スの供給を止め、１８０℃のスチームを供給し脱着した
。Example D MF 1200ppm% M E K 2800E
)I) IR1 Toluene 11000pp 1 Ethyl acetate 1
A model exhaust gas containing 30 ppm was treated with a specific surface area of 1200 m.
'/(ACFCFm adhesion layer 1111 shown in Fig. 1 filled with 3 kg of J acrylic ACF felt in a cylindrical shape)
Supplied in minutes. At this time, since the content of each component in the gas discharged from the ACFCFm layer was 10 ppm or less, the gas was discharged as it was into the atmosphere. Immediately before the MEK content in the emitted gas exceeded 10 ppm, the supply of model exhaust gas was stopped, and steam at 180° C. was supplied for desorption.
脱着スチームを凝縮し、更に分離器にて水層と非水層と
に分離し、水層はＤＭＦを約３％含む水溶液であり活性
炭に通してＤＭＦを吸着させ、塩化メチレンにて脱着及
び蒸留し、ＤＭＦを回収した。その結果ＤＭＦの回収率
は約９２％であった。またＭＥＫ１トルエン及酢酸エチ
ルの回収率は何れも９０％を越えた。The desorption steam is condensed and further separated into an aqueous layer and a non-aqueous layer in a separator. The aqueous layer is an aqueous solution containing about 3% DMF, which is passed through activated carbon to adsorb DMF, and then desorbed and distilled using methylene chloride. Then, DMF was collected. As a result, the recovery rate of DMF was about 92%. Furthermore, the recoveries of MEK1 toluene and ethyl acetate both exceeded 90%.
第１図は本発明に用いられるＡＣＦＣＦｍ着層例を示す
断面図である。FIG. 1 is a sectional view showing an example of ACFCFm layer deposition used in the present invention.
Claims (1)
ムアミドを回収するに当り、該排ガスを繊維状活性炭吸
着層を通してジメチルホルムアミドを吸着除去し、清浄
空気として放出すると共に、ジメチルホルムアミドを吸
着した繊維状活性炭を１６０〜２００℃のスチームにて
脱着することを特徴とするジメチルホルムアミドの回収
方法。In recovering dimethylformamide from exhaust gas containing dimethylformamide, the exhaust gas is passed through a fibrous activated carbon adsorption layer to adsorb and remove dimethylformamide and released as clean air. A method for recovering dimethylformamide, which is characterized by desorption using steam at ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59188896A JPS6168122A (en) | 1984-09-11 | 1984-09-11 | Recovering method of dimethylformamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59188896A JPS6168122A (en) | 1984-09-11 | 1984-09-11 | Recovering method of dimethylformamide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6168122A true JPS6168122A (en) | 1986-04-08 |
| JPH0410368B2 JPH0410368B2 (en) | 1992-02-25 |
Family
ID=16231774
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59188896A Granted JPS6168122A (en) | 1984-09-11 | 1984-09-11 | Recovering method of dimethylformamide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6168122A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6342719A (en) * | 1986-08-08 | 1988-02-23 | Kubota Ltd | Method for deodorizing odorized gas |
| US5908490A (en) * | 1996-05-20 | 1999-06-01 | Toho Chemical Engineering And Construction Co., Ltd. | Organic solvent recovering system and organic solvent recovering method |
| CN103570576A (en) * | 2012-07-20 | 2014-02-12 | 中国石油化工集团公司 | Regeneration system and regeneration method for circulating solvent of cracked C5 separation device |
| CN108976144A (en) * | 2018-08-31 | 2018-12-11 | 潍坊中汇化工有限公司 | A kind of method of biopharmaceutical production DMF waste liquid purification |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5035067A (en) * | 1973-07-24 | 1975-04-03 | ||
| JPS5148769A (en) * | 1974-10-24 | 1976-04-27 | Ota Toshuki |
-
1984
- 1984-09-11 JP JP59188896A patent/JPS6168122A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5035067A (en) * | 1973-07-24 | 1975-04-03 | ||
| JPS5148769A (en) * | 1974-10-24 | 1976-04-27 | Ota Toshuki |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6342719A (en) * | 1986-08-08 | 1988-02-23 | Kubota Ltd | Method for deodorizing odorized gas |
| US5908490A (en) * | 1996-05-20 | 1999-06-01 | Toho Chemical Engineering And Construction Co., Ltd. | Organic solvent recovering system and organic solvent recovering method |
| CN103570576A (en) * | 2012-07-20 | 2014-02-12 | 中国石油化工集团公司 | Regeneration system and regeneration method for circulating solvent of cracked C5 separation device |
| CN108976144A (en) * | 2018-08-31 | 2018-12-11 | 潍坊中汇化工有限公司 | A kind of method of biopharmaceutical production DMF waste liquid purification |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0410368B2 (en) | 1992-02-25 |
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|---|---|---|---|
| EXPY | Cancellation because of completion of term |